JPS5918605A - Manufacture of corrosion-proof iron powder for magnetic recording - Google Patents
Manufacture of corrosion-proof iron powder for magnetic recordingInfo
- Publication number
- JPS5918605A JPS5918605A JP57127469A JP12746982A JPS5918605A JP S5918605 A JPS5918605 A JP S5918605A JP 57127469 A JP57127469 A JP 57127469A JP 12746982 A JP12746982 A JP 12746982A JP S5918605 A JPS5918605 A JP S5918605A
- Authority
- JP
- Japan
- Prior art keywords
- iron powder
- oxide
- ferric
- magnetic iron
- reduction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/06—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/061—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder with a protective layer
Abstract
Description
【発明の詳細な説明】
本発明は分散性、配向性が優れ且つ耐食性が優れた磁気
記録材料用鉄粉の製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing iron powder for magnetic recording materials that has excellent dispersibility, orientation, and corrosion resistance.
高密度記録用の磁性材料として磁性鉄粉が注目されてい
るが、磁性鉄粉は従来から用いられてきた磁性酸化鉄粉
に較べて還元度合が高く、本質的に磁性酸化鉄粉に較べ
て銹びやすい。従って該磁性鉄粉を用いて作った磁気記
録用のテープは経時的に劣化してゆき、記録の長期保持
の点で問題となっているのが現状である。Magnetic iron powder is attracting attention as a magnetic material for high-density recording, but magnetic iron powder has a higher degree of reduction than the conventionally used magnetic iron oxide powder, and is essentially less effective than magnetic iron oxide powder. Easy to rust. Therefore, magnetic recording tapes made using the magnetic iron powder deteriorate over time, posing a problem in terms of long-term retention of records.
磁性鉄粉の耐食性改善の試みは多方面からなされている
が、磁性鉄粉自体に耐食性改善を施すのが最も効果が太
きいと目されている。具体的には還元して得た磁性鉄粉
にＣｒ、 Ａｔ、 ８％を被覆する例、還元前の段階で
磁性鉄粉の前駆体にＣｒ。Attempts to improve the corrosion resistance of magnetic iron powder have been made from various angles, but improving the corrosion resistance of the magnetic iron powder itself is considered to be most effective. Specifically, the magnetic iron powder obtained by reduction is coated with 8% Cr, At, and the precursor of the magnetic iron powder is coated with Cr before reduction.
Ｎｉ 、 Ｂ、 Ｓｉ、 Ａｔ等の成分を添加する°例
等が試みられているがそのいずれの試みもきわだ９た耐
食性を得るには至っていない。Attempts have been made to add components such as Ni, B, Si, At, etc., but none of these attempts have resulted in outstanding corrosion resistance.
本発明者は磁性鉄粉の耐食性向上について検討を行ない
還元前の磁性鉄粉前駆体である針状酸化鉄又は針状含水
酸化鉄の表面（／ｃシリカをＳｉ／Ｆｅの重量比にして
１．５／１００以上を被着させ、該被着量を焼成、還元
すれば、得られた磁性鉄粉の耐食性がきわめて秀れてい
る事を知った。The present inventor investigated the improvement of the corrosion resistance of magnetic iron powder and found that the surface of acicular iron oxide or acicular hydrated iron oxide, which is a magnetic iron powder precursor before reduction (/c silica in the weight ratio of Si/Fe, It has been learned that if an amount of .5/100 or more is deposited and the deposited amount is sintered and reduced, the resulting magnetic iron powder has extremely excellent corrosion resistance.
しかし、この場合の欠点はシリカ被着量の増加とともに
還元速度が後記参考例に示すように減少し、工業的に実
施するには焼成、還元に高温および長時間を要し不経済
であることも同時に知った。However, the drawback in this case is that as the amount of silica deposit increases, the reduction rate decreases as shown in the reference example below, and it is uneconomical to carry out industrially because it requires high temperature and long time for calcination and reduction. I also learned at the same time.
そこで発明者らはＳｉを多く添加することによる耐食効
果を損わずかつ工業的に経済的に焼成、還元できる方法
について詳細に検討したところ更に特定量のＮｉおよび
Ｃｕの添加が有効であることを発見し、本発明を完成し
た。Therefore, the inventors conducted a detailed study on a method that could be industrially and economically fired and reduced without impairing the corrosion resistance effect of adding a large amount of Si, and found that addition of specific amounts of Ni and Cu was effective. discovered and completed the present invention.
ＮｉおよびＣｕの特定の添加量はＮｉ単独の場合にＮｉ
／Ｓｉの重量比にして１〜５の範囲が好ましい事がわか
った一１以下では、工業的に実用可能な還元速度が得ら
れず、５以上とすると磁気特性のうち飽和磁化量（σ８
）が低下するために好ましくない。The specific addition amounts of Ni and Cu are as follows:
/Si weight ratio was found to be preferably in the range of 1 to 5. If it is less than 11, an industrially practical reduction rate cannot be obtained, and if it is more than 5, the saturation magnetization (σ
) is unfavorable because it reduces
Ｃｕ単独の場合もＣｕ／Ｓｉの重量比は１〜５の範囲が
好ましい。理由はＮｉの場合と同様である。Even when Cu is used alone, the weight ratio of Cu/Si is preferably in the range of 1 to 5. The reason is the same as in the case of Ni.
そしてＮｉとＣｕの混合物の場合でも（Ｎｉ＋Ｃｕ）／
Ｓｉの重量比は矢張り１〜５の範囲が好ましい。理由は
Ｎｉ及びＣｕの場合と同様である。And even in the case of a mixture of Ni and Cu (Ni+Cu)/
The weight ratio of Si is preferably in the range of 1 to 5. The reason is the same as in the case of Ni and Cu.
Ｓｉ％Ｎｉ及びＣｕの被着方法について述べるとＳｉ源
としては、水ガラス、コロイダルシリカ各軸のケイ酸塩
等から適宜選定すれば良い。この被着方法としては磁性
鉄粉前駆体である含水酸化鉄又は酸化鉄のスラリー又は
ペーストに上記のＳｉ 源を添加して攪拌又は混練し
、必要においてはその後水洗を行なえば良い。Regarding the method of depositing Si%Ni and Cu, the Si source may be appropriately selected from water glass, colloidal silica silicates, etc. As for this deposition method, the above-mentioned Si source is added to a slurry or paste of hydrated iron oxide or iron oxide, which is a magnetic iron powder precursor, and the mixture is stirred or kneaded, followed by washing with water if necessary.
ＮｉおよびＣｕについて述べると、Ｎｉ 、 Ｃｕ源と
して各々の水可溶性塩が使い易いが水酸化物、酸化物等
の難溶性塩もしくは不溶性塩でも本発明が実施できない
ことはない。これらの被着方法としては前述したＳｉの
被着手法と同様に実施することも出来るが磁性鉄粉前駆
体である含水酸化鉄又は酸化鉄の水懸濁スラリーにＮｉ
又はＣｕの水可溶性ノνカソ
塩を添加し、アジり蝮にて水酸化物に変性する方法が最
も好ましい。この場合アルカリとして苛性ソーダ、苛性
カリ等が使用出来るのはもちろんのこと、水ガラスのア
ルカリ性を利用しても良い。Regarding Ni and Cu, water-soluble salts of each are easy to use as sources of Ni and Cu, but the present invention cannot be practiced using sparingly soluble salts or insoluble salts such as hydroxides and oxides. These deposition methods can be carried out in the same manner as the Si deposition method described above, but Ni
Alternatively, the most preferable method is to add a water-soluble non-v caso salt of Cu and modify it into a hydroxide using an aphrodisiac. In this case, caustic soda, caustic potash, etc. can be used as the alkali, and the alkalinity of water glass may also be used.
Ｎｉ％Ｃｕの被着時期はシリカ被着の前、後、シリカと
の同時被着のいずれでもよい。Ni%Cu may be applied before, after, or simultaneously with silica.
以上のようにして被着した磁性鉄粉前、躯体は５００〜
８５０℃の範囲内で焼成した後、Ｎ２にて３５０〜５５
０℃に於て還元し、該還元鉄粉を非酸化性雰囲気中にて
トルエン等の有機溶剤に浸漬し、次に空気中に取シ出し
て風乾させ、磁性鉄粉を得ることかできる。又、該還元
鉄粉を１００℃以下の温度にて、Ｎ２等の非酸化性ガス
で希釈した空気と接触せしめ該還元鉄粉の表面に酸化被
膜を形成させることにより磁性鉄粉を得ることができる
。Before the magnetic iron powder was deposited as described above, the main body was 500~
After firing within the range of 850℃, 350~55℃ with N2
Magnetic iron powder can be obtained by reducing at 0° C., immersing the reduced iron powder in an organic solvent such as toluene in a non-oxidizing atmosphere, and then taking it out into the air and air drying it. Furthermore, magnetic iron powder can be obtained by contacting the reduced iron powder with air diluted with a non-oxidizing gas such as N2 at a temperature of 100° C. or less to form an oxide film on the surface of the reduced iron powder. can.
これら被着酸化鉄の焼成および還元には公知の方法が適
用できる。Known methods can be applied to firing and reducing the deposited iron oxide.
参考例（Ｓｉのみを被着した実験、実験Ｎ［Ｌｌ−９）
比表面積３５ｍ２／グ、結晶の軸比１０のゲーサイト（
ａ−Ｆｅ００Ｈ）１０グ、水１ｔからなる水懸濁スラリ
ーを調合した。Reference example (experiment in which only Si was deposited, experiment N [Ll-9)
Goethite with a specific surface area of 35 m2/g and a crystal axial ratio of 10 (
A water suspension slurry consisting of 10 g of a-Fe00H) and 1 t of water was prepared.
該水懸濁スラリーに３号水ガラスを添加して攪拌した後
ｐ過、水洗し得られた被着含水ケーキを乾燥して表−１
に示すようにシリカレベルの異なる３種の被着量を得た
。被着量を７００℃の温度に保ったマツフル炉に入れ４
時間焼成したのち、４００℃、４５０℃、５００℃の三
種類の温度にて水素還元を施した。還元後、放冷して還
元粉をＮ２雰囲気中でトルエンに浸漬し、次に空気中に
てトルエンを蒸散させて磁性鉄粉を得た。After adding No. 3 water glass to the water suspension slurry and stirring, it was filtered through p filter and washed with water, and the resulting adhered water-containing cake was dried.
As shown in Figure 3, three types of coatings with different silica levels were obtained. Place the coating in a Matsufuru furnace where the temperature is kept at 700℃ 4
After firing for an hour, hydrogen reduction was performed at three temperatures: 400°C, 450°C, and 500°C. After reduction, the reduced powder was left to cool and immersed in toluene in an N2 atmosphere, and then the toluene was evaporated in air to obtain magnetic iron powder.
耐食性を見るため、磁性鉄粉を６０℃、相対湿度９０％
に保った空気中に１週間放置し、放置前後の０８の変化
を調べた。結果を一括して表１に示す。表１の結果は以
下の如く要約できる。To check corrosion resistance, magnetic iron powder was heated at 60℃ and relative humidity 90%.
The sample was left in an air maintained at a constant temperature for one week, and the changes in 08 before and after being left were examined. The results are summarized in Table 1. The results in Table 1 can be summarized as follows.
シリカ被着量と還元速度の関係についてはシリカの被着
率の増加とともに還元速度が著しく小さくなるのが判る
。特に実験Ｎα４．７．８は還元時間１０．５時間でも
還元不十分であり従ってＨｃ、σ８のレベルが低い。Regarding the relationship between the amount of silica deposited and the reduction rate, it can be seen that the reduction rate decreases significantly as the silica deposition rate increases. In particular, in experiment Nα4.7.8, the reduction was insufficient even after a reduction time of 10.5 hours, and therefore the levels of Hc and σ8 were low.
シリカ被着量と耐食性の関係については還元が十分に進
行した実験例（Ｎ［Ｌ １．２．３．５．６．９）につ
いて見るとシリカ被着量が大きい程耐食性（６０℃相対
湿度９０％にて１週間放置する前後のσ５の差及び放置
後のσＳレベル）が向上しており、シリカ添加量として
Ｓ Ｌ／Ｆ ｅ比にして１．５／１００以上が好ましい
ことが判る。Regarding the relationship between the amount of silica deposited and corrosion resistance, when looking at the experimental example in which reduction had sufficiently progressed (N[L 1.2.3.5.6.9), the larger the amount of silica deposited, the better the corrosion resistance (60℃ relative humidity At 90%, the difference in σ5 before and after leaving for one week and the σS level after leaving were improved, and it is clear that the amount of silica added is preferably 1.5/100 or more in terms of S L /Fe ratio.
実施例（本発明の実施。実験Ｎα１０〜１８）比表面積
３５ ｍ２／７ 、結晶の軸比１ｏのゲーザイ） ］
０ ？、水１ｔからなる水懸濁スラリーを調合した。Example (Implementation of the present invention. Experiment Nα10 to 18) Specific surface area 35 m2/7, crystal axial ratio 1o crystal)]
0? A water suspension slurry consisting of 1 ton of water was prepared.
該水懸濁スラリーに硝酸ニッケル、硝酸銅を添加し、次
いで３号水ガラスを添加し、最終ｐＨが８．０になるよ
うに１Ｎの硝酸及びＩＮの苛性ソーダ水溶液を適量添加
した。Nickel nitrate and copper nitrate were added to the water suspension slurry, then No. 3 water glass was added, and appropriate amounts of 1N nitric acid and IN caustic soda aqueous solution were added so that the final pH was 8.0.
次に該スラリーを濾過、水洗し、得られた被着含水ケー
キを乾燥して被着物を得た。この場合、添加薬剤の量を
調整して表−２に示すような３種類の被着物を得て、こ
れらをそれぞれ実験Ｎ１１ｌＯ〜１２．１３〜１５およ
び１６〜１８に用いた。Next, the slurry was filtered and washed with water, and the resulting adhered water-containing cake was dried to obtain a adherend. In this case, the amount of added chemicals was adjusted to obtain three types of deposits as shown in Table 2, and these were used in experiments N111O~12.13-15 and 16-18, respectively.
被着物を７００’Ｃに保ったマツフル炉に入れ４時間焼
成した後４００，４５０．５００℃の三種類の温度にて
水素還元を施した。The deposit was placed in a Matsufuru furnace kept at 700'C and fired for 4 hours, and then subjected to hydrogen reduction at three different temperatures: 400, 450, and 500C.
還元後は参考例と同様に処理した。結果を表−２に一括
して示す。After reduction, it was treated in the same manner as in the reference example. The results are summarized in Table 2.
表−２の結果は以下の如く要約できる。The results in Table 2 can be summarized as follows.
Ｎｉ及びＣｕの添加により還元速度が大きくなっている
事が参考例と比較すれば明白でありそして磁性鉄粉の耐
食性はシリカの添加量がＳ ｉ／Ｆ ｅにして１．５／
１００以上において十分に発現している。It is clear when compared with the reference example that the reduction rate increases due to the addition of Ni and Cu, and the corrosion resistance of the magnetic iron powder is as follows: the amount of silica added is 1.5/Si/Fe
100 or more, it is sufficiently expressed.
比較例（実験随１９〜２１）
実施例における添加薬剤の量を調整して、本発明で特定
する範囲を外した被着物を得て、実施例と全く同様に処
理して耐食性を調べた。結果をまとめて表３に示したと
うり（Ｎｉ＋Ｃｕ）イＳｉの比が１．０以下では還元速
度が小さく、又（Ｎｉ十Ｃｕ）／Ｓｉの比が５以上では
磁気特性が悪くなることが認められた。Comparative Example (Experiments 19 to 21) By adjusting the amount of the additive agent in the Example, adherends outside the range specified in the present invention were obtained, and treated in exactly the same manner as in the Example to examine corrosion resistance. The results are summarized in Table 3, and it was found that when the (Ni+Cu)/Si ratio is less than 1.0, the reduction rate is low, and when the (Ni+Cu)/Si ratio is 5 or more, the magnetic properties deteriorate. It was done.
Claims (2)
を（Ｎｉ ＋Ｃｕ）／Ｓｉの重量比で１〜５の範囲で被
着後、焼成、還元することを特徴とする耐食性磁気記録
用鉄粉の製造法。(1) Hydrous iron oxide or iron oxide with 5t1Ni and Cu
A method for producing corrosion-resistant magnetic recording iron powder, which comprises depositing (Ni + Cu)/Si at a weight ratio of 1 to 5, followed by firing and reducing.
５Ｘ１°Ｃｒ″２以上としたことを特徴とする特許請求
の範囲第１項に記載の方法。(2) The amount of St deposited is 1.5% by weight ratio of S and i/Fe.
The method according to claim 1, characterized in that the temperature is 5×1°Cr″2 or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57127469A JPS5918605A (en) | 1982-07-23 | 1982-07-23 | Manufacture of corrosion-proof iron powder for magnetic recording |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57127469A JPS5918605A (en) | 1982-07-23 | 1982-07-23 | Manufacture of corrosion-proof iron powder for magnetic recording |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5918605A true JPS5918605A (en) | 1984-01-31 |
| JPH0334641B2 JPH0334641B2 (en) | 1991-05-23 |
Family
ID=14960693
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57127469A Granted JPS5918605A (en) | 1982-07-23 | 1982-07-23 | Manufacture of corrosion-proof iron powder for magnetic recording |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5918605A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS619553A (en) * | 1984-06-25 | 1986-01-17 | Kanto Denka Kogyo Kk | Magnetic powder and its manufacture |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56156706A (en) * | 1980-05-06 | 1981-12-03 | Hitachi Maxell Ltd | Manufacture of magnetic metallic powder |
-
1982
- 1982-07-23 JP JP57127469A patent/JPS5918605A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56156706A (en) * | 1980-05-06 | 1981-12-03 | Hitachi Maxell Ltd | Manufacture of magnetic metallic powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS619553A (en) * | 1984-06-25 | 1986-01-17 | Kanto Denka Kogyo Kk | Magnetic powder and its manufacture |
| JPH0312125B2 (en) * | 1984-06-25 | 1991-02-19 | Kanto Denka Kogyo Kk |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0334641B2 (en) | 1991-05-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPS6348810B2 (en) | ||
| JPS6044805B2 (en) | Method for manufacturing magnetic recording media | |
| JPS5918605A (en) | Manufacture of corrosion-proof iron powder for magnetic recording | |
| JPS59107924A (en) | Manufacture of magnetic iron oxide powder containing cobalt | |
| JPS5919163B2 (en) | Method for producing magnetic metal powder | |
| JPS62241827A (en) | Production of ferromagnetic fine powder for magnetic recording | |
| JPS5919168B2 (en) | Manufacturing method of metal magnetic powder | |
| JPS5919169B2 (en) | Manufacturing method of metal magnetic powder | |
| JPS6217364B2 (en) | ||
| JPH0420241B2 (en) | ||
| JPS6122604A (en) | Magnetic metal powder and manufacture thereof | |
| JPH02175806A (en) | Manufacture of metal magnetic powder for magnetic recorder | |
| JPH0283219A (en) | Production of cobalt-containing ferromagnetic iron oxide powder | |
| JPS6259531A (en) | Production of barium ferrite powder | |
| JPS6346961B2 (en) | ||
| JPS6110031A (en) | Improved multilayer process for cobalt treatment of ferromagnetic oxide | |
| JPS61160905A (en) | Magnetic metal powder | |
| JPS62219902A (en) | Manufacture of metal magnetic powder | |
| JPS62156209A (en) | Ferromagnetic metallic powder | |
| JPS58161709A (en) | Production of magnetic metallic iron powder | |
| JPS59170209A (en) | Production of magnetic metallic powder for magnetic recording | |
| JPS63183616A (en) | Magnetic powder for magnetic recording medium | |
| JPS60114509A (en) | Manufacture of magnetic powder | |
| JPS63265823A (en) | Method for coating metal compound on fine particles of acicular iron oxyhydroxide or the like | |
| JPS61186401A (en) | Ferromagnetic metallic powder and its production |